US11092533B2 - Method for measuring undissolved material in polymer solution - Google Patents

Method for measuring undissolved material in polymer solution Download PDF

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Publication number
US11092533B2
US11092533B2 US16/767,166 US201916767166A US11092533B2 US 11092533 B2 US11092533 B2 US 11092533B2 US 201916767166 A US201916767166 A US 201916767166A US 11092533 B2 US11092533 B2 US 11092533B2
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polymer solution
transparent plate
undissolved substances
light source
light
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US20200386663A1 (en
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Hwi Soo YANG
Ga Hyun LIM
Sang Hoon Choy
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LG Energy Solution Ltd
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LG Chem Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G01N15/0205—Investigating particle size or size distribution by optical means
    • G01N15/0227—Investigating particle size or size distribution by optical means using imaging; using holography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/02—Investigating particle size or size distribution
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/10—Investigating individual particles
    • G01N2015/1029—Particle size
    • G01N2015/1087—
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a method for measuring undissolved substances of a polymer solution used in preparing an electrode slurry.
  • secondary batteries capable of charging and discharging have been widely used as energy sources of wireless mobile devices.
  • the secondary battery has attracted attention as an energy source of an electric vehicle, a hybrid electric vehicle, etc., which are proposed as a solution for air pollution of existing gasoline vehicles and diesel vehicles using fossil fuel. Therefore, the types of applications using the secondary battery are currently much diversified due to the advantages of the secondary battery, and it is expected that the secondary battery will be applied to many fields and products in the future.
  • the secondary battery is formed by inserting an electrode assembly including a positive electrode, a separator, and a negative electrode in a pouch and injecting electrolyte therein.
  • the positive electrode and the negative electrode constituting the electrode assembly of the secondary battery are formed by applying a positive electrode active material and a negative electrode active material on an electrode sheet.
  • a lithium cobalt oxide, a lithium manganese oxide, a lithium nickel oxide, a lithium composite oxide, and the like are used as positive electrode active materials of the lithium secondary battery, and carbon materials are mainly used as negative electrode active materials and the use of silicon compounds and sulfur compounds as negative electrode active materials is also considered.
  • a slurry is prepared by dispersing an active material, a conductive material, a binder, and the like in a solvent. Therefore, the slurry is directly applied to the electrode current collector and dried to thereby form an electrode of the secondary battery. Alternatively, the slurry is applied on the upper part of a separate support and dried, and then a film peeled from the support is laminated on the current collector to thereby form an electrode of a secondary battery.
  • a method of measuring undissolved substances is to apply a solution to a plate 10 with a blade and measure the number of gels 21 shown in the applied solution 20 in the light 30 .
  • the measurement method is different in its standard according to the measuring person, and measurement errors may occur even when the measurement is performed by the same person.
  • the measurement method has a disadvantage in that the size of the gel by the undissolved substances cannot be measured, and thus there is a limit in determining whether the performance of the battery by the undissolved substances is lowered when an actual electrode is manufactured.
  • an object of the present invention is to provide a method for measuring undissolved substances of a polymer solution, and more particularly, to provide a method for effectively measuring the number and size of gels by the undissolved substances by scraping and applying the polymer solution using a blade having a fixed interval, supplying light from the bottom and, at the same time, photographing the shape of light having passed through the solution from the top.
  • the method for measuring undissolved substances of a polymer solution for achieving the above object may include a solution application step of applying a polymer solution on a transparent plate; a light supplying step of supplying light to the polymer solution applied on the transparent plate by a light source; a photographing step of photographing a shape of the light having penetrated the polymer solution applied on the transparent plate; and a measuring step of checking a number and a particle size of undissolved substances in the polymer solution with the photographed image.
  • the polymer solution may be a polymer solution for preparing an electrode slurry of a secondary battery.
  • the minimum measurable particle diameter of the undissolved substances may be 100 ⁇ m.
  • the transparent plate may be made of OHP or glass.
  • the solution can be applied by scraping the polymer solution with a blade.
  • the gap from the transparent plate to the blade may be 80 to 200 ⁇ m, more preferably 100 to 150 ⁇ m, most preferably 110 ⁇ m to 140 ⁇ m.
  • the light source may be located under the transparent plate.
  • the light source may be a planar surface light source.
  • the surface light source of the present invention may include the pattern for measuring the number and diameter of undissolved substances of the polymer solution on the upper part of the surface emitting light.
  • the illuminance of the light source may be 750 to 1250 lux, more preferably 900 to 1100 lux.
  • the photographing may be performed at an upper portion of the transparent plate.
  • the method of measuring undissolved substances of a polymer solution according to the present invention has an effect of objectively measuring the size and number of gels by the undissolved substances of the polymer solution when preparing an electrode slurry through an image photographed by a test device.
  • the method of measuring the undissolved substances of the polymer solution according to the present invention enables effective management of the undissolved substances in the prepared polymer solution for the slurry, thereby preventing the surface defect of the electrode and an increase in the resistance of the battery cell.
  • FIG. 1 is a schematic diagram showing a conventional method for measuring the number of undissolved substances when preparing a slurry.
  • FIG. 2 is a perspective view showing the relative positions of a transparent plate, a pattern for measuring undissolved substances, and a light source in a method for measuring undissolved substances according to an embodiment of the present invention.
  • FIG. 3 is a side view showing a measurement when there is no undissolved substance in a polymer solution using a undissolved substance measurement method of a polymer solution according to an embodiment of the present invention.
  • FIG. 4 is a side view showing a measurement when there is are undissolved substances in a polymer solution using a undissolved substance measurement method of a polymer solution according to an embodiment of the present invention.
  • FIG. 5 shows an image of a polymer solution taken according to an embodiment of the present invention.
  • FIG. 6 shows an image converted by adjusting the brightness contrast of the image of FIG. 5 photographed according to an embodiment of the present invention.
  • FIG. 7 is a flowchart showing the procedure of a method for measuring undissolved substances of a polymer solution of the present invention.
  • the method for measuring the undissolved substances of a polymer solution of the present invention may include: a solution application step of applying a polymer solution on a transparent plate 100 (S 1 ); a light supplying step of supplying light to the polymer solution applied on the transparent plate 100 by a light source 300 (S 2 ); a photographing step of photographing a shape of the light having penetrated the polymer solution 200 applied on the transparent plate 100 (S 3 ); and a measuring step of checking a number and a particle size of undissolved substances in the polymer solution with the photographed image (S 4 ).
  • any transparent material through which light is transmitted may be used as the material of the transparent plate 100 , but the material is preferably OHP or glass.
  • the polymer solution is evenly applied to the transparent plate 100 .
  • the transparent plate 100 should maintain a horizontal state with the ground in order to maintain the state of the applied polymer solution 200 .
  • the polymer solution may be a polymer solution for an electrode slurry for manufacturing a positive electrode or a negative electrode.
  • the polymer solution for the electrode slurry may be a thickener or binder solution used in preparing the electrode slurry.
  • the thickener may be one or more selected from the group consisting of Carboxymethyl cellulose (CMC), methyl cellulose (MC), hydroxypropyl cellulose (HPC), methyl hydroxypropyl cellulose (MHPC), ethyl hydroxyethyl cellulose (EHEC), methyl ethyl hydroxyethyl cellulose (MEHEC) and cellulose gum.
  • CMC Carboxymethyl cellulose
  • MC methyl cellulose
  • HPC hydroxypropyl cellulose
  • MHPC methyl hydroxypropyl cellulose
  • EHEC ethyl hydroxyethyl cellulose
  • MEHEC methyl ethyl hydroxyethyl cellulose
  • the binder may be one or more selected from the group consisting of styrene-butadiene rubber (SBR), polyvinylidene fluoride (PVdF), copolymer of polyhexafluoropropylene-polyvinylidene fluoride (PVdF/HFP), poly (vinylacetate), polyvinyl alcohol, polyethylene oxide, polyvinylpyrrolidone, alkylated polyethylene oxide, polyvinyl ether, poly (methyl methacrylate), poly (ethylacrylate), polytetrafluoroethylene (PTFE), polyvinylchloride, polyacrylonitrile, polyvinylpyridine, acrylonitrile-butadiene rubber and ethylene propylene diene monomer (EPDM).
  • SBR styrene-butadiene rubber
  • PVdF polyvinylidene fluoride
  • PVdF/HFP copolymer of polyhexafluoropropylene-pol
  • the number and particle diameter of the undissolved substances that may cause surface defects of the electrode and increased resistance of the secondary battery are measured.
  • the minimum measurable particle diameter of the undissolved substances may be 100 ⁇ m.
  • the solution can be applied by scraping the polymer solution with a blade.
  • the application of the polymer solution should be made so that the light transmission is effective in the portion of the polymer solution where the undissolved substances do not exist, and the refraction of the light may be sufficiently observed in the portion of the polymer solution in which the undissolved substances exist.
  • the gap from the transparent plate 100 to the blade may be 80 to 200 ⁇ m, more preferably 100 to 150 ⁇ m, most preferably 110 ⁇ m to 140 ⁇ m.
  • the gap from the transparent plate to the blade means the distance from the transparent plate to the blade edge.
  • the distance from the transparent plate to the blade is less than 80 ⁇ m, a hole may occur depending on the viscosity, and when the size of the undissolved substance is large, there is a problem that it is difficult to observe the refraction of light by scratching the surface.
  • the distance from the transparent plate to the blade exceeds 200 ⁇ m and the coating is too thick, the undissolved substances may not be sufficiently detected, and therefore it is preferable to adjust the distance from the transparent plate to the blade to 80 to 200 ⁇ m for relative comparison between test samples.
  • the light source 300 may be located below the transparent plate.
  • the light source 300 can supply light evenly to the polymer solution 200 applied to the transparent plate 100 , but the light source is preferably a planar surface light source which evenly supplies light to all areas of the applied polymer solution 200 .
  • the planar surface light source of the present invention may include a pattern 310 for measuring the undissolved substances for measuring the number of undissolved substances of the polymer solution and the area on the upper part of the surface emitting light.
  • the pattern 310 for measuring the undissolved substances may be a pattern of a predetermined size printed on a transparent material that can transmit light, preferably a circular pattern for accurate measurement.
  • the light emitted from the light source 300 in the light supplying step (S 2 ) of the present invention passes through the pattern 310 for measuring the undissolved substances, the transparent plate 100 , and the applied polymer solution 200 in order.
  • the illuminance of the light source 300 is sufficient if it can sufficiently pass through the pattern 310 for measuring the undissolved substances, the transparent plate 100 , and the applied polymer solution 200 .
  • it may be 750 to 1250 lux, more preferably 900 to 1100 lux.
  • the surface of the solution remains evenly flat.
  • the light emitted from the light source 300 passes through the portion having no undissolved substance, it passes through a path 301 without refraction.
  • the light transmitted through the path 301 without refraction shows a shape 400 which projects the pattern 310 for measuring the undissolved substances as it is.
  • the light emitted from the light source 300 passes through the portion having no undissolved substance, it passes through a path 301 without refraction.
  • Part of the light emitted from the light source is transmitted through a path (divergence, 302 ) refracted at the surface of the solution due to the bend 210 of the solution surface when there are undissolved substances in the applied polymer solution 200 .
  • Part of the light emitted from the light source is transmitted through a path (total reflection, 303 ) totally reflected at the surface of the solution due to the bend 210 of the solution surface when there are undissolved substances in the applied polymer solution 200 .
  • the light transmitted through the path 301 without refraction shows a shape 400 which projects the pattern 310 for measuring the undissolved substances as it is.
  • the light transmitted through the refracting path 302 ambiguously projects the pattern 310 for measuring undissolved substances.
  • the light transmitted through the completely reflecting path 303 does not project the pattern 310 for measuring the undissolved substances.
  • a circular pattern is generally present in the background, and a blurred area covering the circular pattern is present in some places.
  • the blurred area is an image which is generated as light irradiated from a light source is refracted by the bending of undissolved substances.
  • the size of the pattern formed on the image is smaller than the size of the blurred area. Therefore, it is preferable that the size of the pattern formed on an image is equal to or less than 100 micrometers which is a minimum diameter which can be measured.
  • the size of the pattern formed on the image can be adjusted by appropriately selecting the distance between the light source and the transparent plate. In one embodiment of the present invention, in order to adjust the size of the pattern formed on the image to 80 ⁇ m or less, the distance between the light source and the transparent plate was adjusted to a length of 0.3 to 1 meters.
  • the photographing may be performed at an upper portion of the transparent plate.
  • the light emitted from the light source penetrates the pattern 310 for measuring the undissolved substances, the transparent plate 100 , and the applied polymer solution 200 through the path 301 without refraction, the refracting path 302 , and the completely reflecting path 303 .
  • the light transmitted through the refracting path 302 ambiguously projects the pattern 310 for measuring undissolved substances.
  • the light transmitted through the completely reflecting path 303 does not project the pattern 310 for measuring the undissolved substances.
  • the shape of the projected light is photographed as an image.
  • the image 410 when the undissolved substances exist in the applied polymer solution 200 is the same as the pattern shape of the pattern 310 for measuring the undissolved substances, but the portion where gels by the undissolved substances exist include a shape 411 which the boundary of the pattern is unclear.
  • the number and particle size of the undissolved substances in the polymer solution are checked by analyzing the image photographed in the photographing step (S 3 ).
  • the number and the area (pixel) of the shapes 411 are measured, and they can be converted into the particle diameters of the undissolved substances through the area.
  • the number of shapes 411 of which the boundary of the pattern is unclear means the number of undissolved substances in the polymer solution.
  • the diameter of the shape 411 whose boundary of the pattern is unclear means the particle diameter of the undissolved substances in the polymer solution.
  • An image conversion step of adjusting the contrast of the image may be further included in order to facilitate analysis of the image photographed in the photographing step S 3 before the measuring step S 4 of the present invention.
  • the brightness of the unclear pattern 411 is lowered, so that the difference in brightness from the surrounding image becomes clearer, so that the number and particle size of the undissolved substances can be measured more accurately.
  • a transparent plate of glass material was placed on top of the planar surface light source where the circular pattern was located, and the transparent plate was positioned to be about 1 m away from the planar surface light source, so that the diameter of the circular pattern formed thereon was adjusted to be 80 ⁇ m.
  • the CMC solution (1.0 to 2.0% concentration solution dissolved in distilled water) was applied onto the transparent plate made of glass with a blade keeping a fixed distance of 100 ⁇ m from the transparent plate.
  • FIG. 5 The image of the light emitted from the light source and transmitted through the CMC solution in the light supply step was photographed using the camera located on the transparent plate, and the photographed image is shown in FIG. 5 .
  • the image was converted by adjusting the contrast in order to effectively measure the unclear portion of the photographed image.
  • FIG. 6 shows an image converted from FIG. 5 by emphasizing contrast. As shown in FIGS. 5 and 6 , the brightness of the unclear portion of the image generated by the gel by the undissolved substances in the solution was minimized through the image conversion.
  • a unique number is assigned to each of the parts in which the brightness of the converted image has been minimized, and pixel values of the image are measured for each unique number, and the results are shown in Table 1 below.
  • Example 1 When applying the CMC solution in Example 1, the number and the size of undissolved substances were checked in the same manner as in Example 1 except that the distance between the transparent plate and the blade was adjusted to 150 ⁇ m, and the result was shown in Table 1.
  • Example 2 ID number Pixel ID number Pixel 1 6689 1 2195 2 4709 2 889 3 1292 3 5611 4 1318 4 7367 5 3832 5 604 6 1550 6 1266 7 5438 7 4302 8 2995 8 3804 9 685 9 502 10 1698 10 611 11 507 11 3032 12 570 12 758 13 7311 13 3938 14 928 14 2350 15 8437 15 1212 16 1403 16 2251 17 2426 17 1355 18 996 18 789 19 543 19 1980 20 2296 20 2750 21 7288 22 5051 23 1218
  • the CMC solution used in the above example 1 was checked by naked eyes, and the number of gels by the undissolved substances shown in the applied solution was measured.
  • Example 2 When applying the CMC solution in Example 1, the solution was applied and light was supplied in the same manner as in Example 1 except that the distance between the transparent plate and the blade was adjusted to 250 ⁇ m. After that, it was tried to check the number and size of the undissolved substances, but because the CMC solution is too thick, the undissolved substances were completely covered by the CMC solution, and the number of the undissolved substances was shown as 6.
  • the pattern formed in the image is clearly distinguished from the blurred area, there is an effect that there is no deviation in the number of the undissolved substances according to the testing person.
  • the actual particle size value of the undissolved substances can be calculated based on the pixel value of the blurred area, there is an effect that the particle size of the undissolved substances can be measured.

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KR10-2018-0090666 2018-08-03
KR1020180090666A KR102309284B1 (ko) 2018-08-03 2018-08-03 고분자 솔루션의 미용해물 측정법
PCT/KR2019/009538 WO2020027573A1 (ko) 2018-08-03 2019-07-31 고분자 솔루션의 미용해물 측정법

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